Distilling and rectifying apparatus



juy M, wm A. MA@

nDIS'I'ILLING AND RECTIFYING APPARATUS Filed April 29, 1946 ww. W AM Wm\ 6% www M x rd W MH- m, y u w .WN WM Patented July 24, 1951 2,561,669 DISTILLING AND RECTIFYING APPARATUS Andr Macq, Uccle, Brussels, Belgiumyassignor to' Union Chimique Belge, Socit Anonyme,

` Brussels, Belgium Application April 29, 1946, Serial No. 665,674 In Belgium April 25, 1945 Distillation and rectification columns comprising the usual bell plates or plates with perforated bases have the disadvantage of forming apparatus having a great height. For this reason it is frequently impossible to install the necessary number of plates for enabling mixtures of substances having boiling points which are near each other to be separated satisfactorily, and it is necessary to have recourse yto multiple refiuxes of the materials being treated; this influences the thermal balance of these installations very unfavourably.

The subject matter of the present invention is a distillation and rectification apparatus comprising a column of plates of very small height which enables substances having boiling points which are near each other to be separated whilst reducing the multiple refluxes to such an extent that they are very little in excess of the theoretical value. The small height of the plates enables columns of small bulk to be formed which do Vnot necessitate the construction of special buildings to shelter them. The plates according to the invention are arranged in such a manner that a very sharp separation of the constituents of the mixture treated can be effected without bubbling the vapours in the liquids on the plates. A very low loss of pressure results; this is an advantage which enables the number of plates to be increased, if necessary in certain cases, whilst the height of the column remains considerably below 'the usual height of the columns at present employed. The small height of the column and the insignicant reflux enable an extraordinary thermal yield to be obtained and the consumption n of heating steam to be reduced to a fraction of that ordinarily allowed for columns `with bell plates. These same factors, added to the very thorough separation of the constituents to be rectied and the very small loss of pressure, enable,-in addition, the economical rectification of mixtures of substances of very close boiling points to be envisaged, mixtures for which the separation by distillation and rectification has hitherto not been contemplated and which have had to be subjected to complicated chemical treatments.

The column forming the subject matter of the invention is constituted by identical vertically superposed elements, each of which comprises a fixed part and a movable part. The movable parts of all the elements of a column are fixed on a shaft such as hereinafter described. The attainment of the above and further objects will be apparent from the following specification taken `for the overhead vapours. "cylinder f the shaft i has a reciprocatory and 3 Claims. (Cl. 261-81) in` conjunction with the drawing forming a part thereof.

`In the drawing:

Figure 1 is a longitudinal sectional view of the top of a column, with parts broken away, showing the movable members in their elevated positions; and

Figure 2 is a longitudinal sectional view of the bottom of the same column, with parts broken away showing the movable parts in ltheir lowered position.

Referring now to Figure 1 the fixed part is in the form of a circular plate c which posseses at its centre a wide orifice a that is bounded by a wall or strip b which limits the height of the liquid remaining on the plates. Near the outer edge of this plate there is fixed a cylindrical sheet of metal e on which is placed the upper plate which xes the height of the elements of the column. All the elements of the column are surrounded by a cylinder f, closed at its` two ends and suitably lagged. A packing d may be placed between each of the plates and the cylinder.

The movable part of each element is in the form of a circular imperforate bale plate or `dischl of sheet metal or other suitable material, ithe diameter of which is slightly less than that of the fixed plate, this disc bearing, on its bottom face at a distance of a few millimetres, an annular device with a large surface of contact and retention, which device is formed, for example, by one or more layers of netting and is represented diagrammatically in Figs. 1 and 2 by the broken lines g. The discs of all the elements of a column are fixed in a suitable manner on a vertical shaft z' placed at the axis of the outer cylinder and passing through the central orifices of the plates. Referring now to Figure 1, the end of the shaft i passes through the upper end sof the outer cylinder f. A delivery pipe r is provided Externally .of the `rotary motion imparted thereto by any suitable mechanism indicated by the reference letter m. The effect of these movements is to cause the discs to rise in order to give a full passage to the vapours which rise between the fixed parts and the movable parts of the elements of the column and to cause them to descend until the device with a large surface of contact and of retention, which is xed to the bottom of the discs, is immersed in the descending liquids spread on the plates. Fig. 2 shows the device at the moment of immersion. The bottom t of the column f has a suitable bearing o for the vertical shaft and an inlet p for vapours and an outlet q for reflux.

The very small height of the plates and the movements described of the movable part have the effect of presenting to the vapours very large surfaces, which ,are wetted by the constantly renewed liquids, andiV of enabling multiple exchanges between the vapours and the liquids to take place, thus ensuring the rapid separation of the mixtures being rectified into their components. These circumstances favour vthedi, nglinll151011 ofthe reflux to almost the theoretical value.

The column described may b e vused :both for continuous as well as for discontinuous working. In discontinuous working, the vapours coming from the boiler rise in the column by -Way Q-f' the first plate and meet, in counter-current, the-freuxed liquids which drop fromplate to plate through the Wide central oriiices and which,'in falling, sprinkle the upper faces of the moving discs.Y The vapours lick the liquidson thelplates and on all the very exposed surfaces of themovable partsvas thel result of trickling, wetting vand splashing.. At the periphery of the plates, the vapours undergo Ia change `or direction of 180 and pass into the partiormed by the top of a movable disc and the bottom of the plate above the movable disc where they have the opportun- `ityof leaving the small drops which have -been taken along mechanically or have been `formed by `V`condensation.

In a column ysuch ras the one described, which was equipped for,discontinuous-working and had a useful'height Qi" 15,0 centimetres and comprised 50 plates, 220 kgs. of a'rnixture of benzene and toluene were rectied. rIhe separation of the constituents was extremely sharp. The ratio of reflux to` distillate was-'less than 1 and the loss of pressure uctuatedbetween "120 and 140 mms. of water according to' the momentary position of ,the movable discs; vit therefore d id not exceed 2.8 mms. of water per plate. 1Y0-kgs. ofbenzene, ofa quality superior tothe standards of the Ben- Zol-Verband (Benzene Association) were btained. The jliquid remaining in the boiler did not contain any trace of benzeneand the fraction of V 13.3 kgs. intermediate between benzene and toluene corresponded yto about the 'liquid Vcapacity yof the column.

In continuous working, the liquid to be -rectied Was, as usual, heated to its `boiling pointand introduced on toy an intermediate plate of the column. A result, which Was comparable with that indicated for the discontinuous working, was obtained.

It has also been possible to rectify, With surprising success, in a single operation in thesame column mixtures `in which the boiling points `of the `constii'luents were only 10 C. apart, such as, for example, phenol and orthocresol. working under very favourable `c )-Jf.wl,t r1 s cf economy and avoiding the multiple rectifications withr abundant refluxes which it is necessary to `carry-Out in `plate columns yof the present-day type.

r Number The column described may be employed under any conditions of pressure. The fact that it requires only one fluid-tight joint, which is favourably situated and is of small dimensions, predestines it for employment in vacuo. There may be given to the central orice of the xed plates c a particular shape which increases vthe development of the length ofthe strip b in relation to that which results from the employment of a 'merely circular central orice.

y,The ucolumn described may also be employed advantageously for the washing of industrial gases.

l.In a multpleplate distillation and rectili- ,cation column, the combination of a vertical vcylindrical column wall, a shaft coaxial therewith and `guided for both rotary and reciprocatory movements, means for imparting said movements thereto, a plurality of superimposed annular imperfcrate baille plates peripherally sealed and. -xed upon saidy wall, a plurality `of lvertically spaced circular'imperforate baiile plates coaxially mounted in ysaidsh-aft for rotation and reciprocaftion therewitlfi and alternately interposed between said annular plates; the central aperture in each'of said annularlplates being Ybound 4by an upsta-nding'wall limiting the height of the liquid on theannular-plates, 'a'layer of contact material mounted on -the under side Aof said-circular plates, said material 1providing large surfaces `for vapor contact and liquid retention and adapted to be alternately immersed in the liquid inthe vsub- Yjacent annular plates at the 4lower position of the reciprocable `plates and elevated above the liquid vinthe upper position vof the reciprocable plates, whereby the vapours traverse a generally upward and zig-'Zag path between the circular and annular plates.

L2. Apparatus gas dened in claim l wherein each of said vlayers of Contact material has a thickness only-slightly less than the height of said rupstanding wall.

'3. Apparatus as claimed in claim 1 wherein said annular-plates are closely superimposed and wherein said reciprocable Yplates extend nearly to the outer-periphery-of said annular plates.

ANDRE MACQ.

'REFERENCES CITED ,'Iljle following lreferences are of record in the `,ille of this patenti UNITED STAT-ES PA'FETN'ES Name Date Ledig July 30, 1889 Pegram Oct. 15 V1940 Bottoms et al.Y Oct. 23, 1945i .FOREIGN PATENTS Country Date Great Britain Feb.v 25, 1884 Great Britain Mar. 25, 1911 Number 

